QuEChERS-超高效液相-三重四极杆串联质谱测定白茅根中16种真菌毒素  

Simultaneous determination of sixteen mycotoxins contaminants in cogon rootstalk by QuEChERS-UPLC-QqQ mass spectrometry

作　　者：范妙璇[1] 董娇娇 王京辉[1] 郭洪祝[1] 陈有根[1] 傅欣彤[1] 

机构地区：[1]北京市药品检验所中药成分分析与生物评价北京市重点实验室,北京102206 [2]北京中医药大学中药学院,北京100029

出　　处：《中国中药杂志》2017年第19期3770-3775,共6页China Journal of Chinese Materia Medica

基　　金：中央本级重大增减项目

摘　　要：该文建立了一种同时检测白茅根中16种真菌毒素的QuECh ERS(Quick,Easy,Cheap,Effective,Rugged,Safe)超高效液相色谱串联质谱定量分析方法。白茅根以1%乙酸-乙腈超声提取,QuEChERS方法净化,用甲醇和含0.01%甲酸水溶液为流动相进行梯度洗脱,超高效液相色谱仪应用Agilent Eclipse Plus C_(18)色谱柱,优化选择在电喷雾离子源正离子模式下以多反应监测方式检测。结果表明,16种真菌毒素在各自线性范围内线性关系良好,相关系数r在0.996 2~1.000,定量限为0.03~186.68μg·kg^(-1),回收率为60.28%~129.2%,RSD为0.29%~11%。该方法净化效果好、灵敏度高、重复性好,适用于基质成分复杂的白茅根中多种真菌毒素的定量检测。A method for the simultaneous determination of sixteen mycotoxins in cogon rootstalk was developed using ultra-performance liquid chromatography coupled with triple quadropole mass spectrometry（ UPLC-QqQ-MS/MS）. The samples were extracted with acetonitrile contained 1% acetic acid and purified by QuEChERS method. The separation was performed on an Agilent Eclipse Plus C18 column by gradient elution using methanol and 0. 01% aqueous formic acid as mobile phase. The targeted compounds were detected in MRM mode by mass spectrometry with electrospray ionization（ ESI） source operated in positive ionization mode. The linear relationships of the sixteen mycotoxins were good in their respective linear ranges. The correlation coefficients（ r） ranged among 0. 996 2-1. 000. The LOQs of the sixteen mycotoxins were between 0. 03 and 186. 68 μg·kg^-1. The average recoveries ranged from 60. 28% to 129. 2%with relative standard deviations（ RSDs） within 0. 29%-11%. The results demonstrated that the proposed method was sensitive and accurate,and suitable for the mycotoxins quantification in cogon rootstalk.

关 键 词：真菌毒素 QuEChERS法 超高效液相-三重四级杆联用质谱 白茅根 

分 类 号：O657.63[理学—分析化学] R284.1[理学—化学]